#------------------------------------------------------------------------------
#$Date: 2021-03-18 12:27:51 +0200 (Thu, 18 Mar 2021) $
#$Revision: 263117 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/11/1561115.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1561115
loop_
_publ_author_name
'Huang, Guo-Zhen'
'Zou, Xin'
'Zhu, Zhi-Biao'
'Deng, Zhao-Peng'
'Huo, Li-Hua'
'Gao, Shan'
_publ_section_title
;
 Syntheses and characterizations of secondary Pb--O bonding supported
 Pb(II)-sulfonate complexes
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              214
_journal_page_last               223
_journal_paper_doi               10.1016/j.jssc.2018.03.025
_journal_volume                  262
_journal_year                    2018
_chemical_formula_moiety         'C7 H8 O9 Pb S, C3 H7 N O, H2 O'
_chemical_formula_sum            'C10 H17 N O11 Pb S'
_chemical_formula_weight         566.50
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                98.376(4)
_cell_angle_beta                 100.877(4)
_cell_angle_gamma                106.094(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4170(4)
_cell_length_b                   8.6990(4)
_cell_length_c                   12.2865(7)
_cell_measurement_reflns_used    2875
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.88
_cell_measurement_theta_min      3.31
_cell_volume                     829.93(8)
_computing_cell_refinement
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis Pro (Agilent, 2013)
;
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 16.1954
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5136
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    10.347
_exptl_absorpt_correction_T_max  0.3699
_exptl_absorpt_correction_T_min  0.2199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.827
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       0.0032(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         2913
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0402P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                2733
_reflns_number_total             2913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2018-262-214.cif
_cod_data_source_block           complex6
_cod_original_cell_volume        829.93(7)
_cod_database_code               1561115
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.70416(3) 0.87472(3) 0.51208(2) 0.02379(13) Uani 1 1 d . . .
S1 S 0.9125(2) 0.76329(19) 0.27469(15) 0.0272(4) Uani 1 1 d . . .
O1 O 0.9433(6) 0.8837(5) 0.3787(4) 0.0318(11) Uani 1 1 d . . .
O1W O 0.5274(7) 0.8088(7) 0.3180(4) 0.0395(12) Uani 1 1 d D . .
H1W1 H 0.595(8) 0.797(10) 0.277(5) 0.059 Uiso 1 1 d D . .
H1W2 H 0.467(9) 0.864(9) 0.291(6) 0.059 Uiso 1 1 d D . .
O2 O 1.0477(7) 0.8016(6) 0.2159(5) 0.0451(14) Uani 1 1 d . . .
O2W O 0.6444(7) 0.9751(7) 0.7224(5) 0.0490(14) Uani 1 1 d . . .
H2W2 H 0.6092 0.9294 0.7737 0.074 Uiso 1 1 d R . .
H2W1 H 0.7431 1.0434 0.7513 0.074 Uiso 1 1 d R . .
O3 O 0.7460(6) 0.7325(6) 0.2011(4) 0.0388(12) Uani 1 1 d . . .
O3W O 0.6442(7) 0.5603(7) 0.8033(5) 0.0584(16) Uani 1 1 d . . .
H3W2 H 0.6174 0.6414 0.8327 0.088 Uiso 1 1 d R . .
H3W1 H 0.5652 0.5067 0.7452 0.088 Uiso 1 1 d R . .
O4 O 0.6784(5) 0.5810(5) 0.3956(4) 0.0252(10) Uani 1 1 d D . .
H4O H 0.603(7) 0.510(7) 0.415(6) 0.038 Uiso 1 1 d D . .
O5 O 0.5433(5) 0.3414(5) 0.4715(4) 0.0329(11) Uani 1 1 d . . .
O6 O 0.6522(6) 0.1416(6) 0.4873(5) 0.0361(12) Uani 1 1 d . . .
O7 O 1.1648(6) 0.2921(6) 0.3234(5) 0.0343(11) Uani 1 1 d D . .
H7O H 1.225(9) 0.339(9) 0.282(6) 0.051 Uiso 1 1 d D . .
O8 O 0.4945(9) 0.8053(11) 0.8640(7) 0.090(2) Uani 1 1 d . . .
N1 N 0.2649(11) 0.7935(13) 0.9380(7) 0.076(3) Uani 1 1 d . . .
C1 C 0.9167(8) 0.5792(7) 0.3191(5) 0.0215(13) Uani 1 1 d . . .
C2 C 0.7947(7) 0.5057(7) 0.3744(5) 0.0175(12) Uani 1 1 d . . .
C3 C 0.7925(7) 0.3592(7) 0.4061(5) 0.0194(13) Uani 1 1 d . . .
C4 C 0.9179(7) 0.2908(7) 0.3868(5) 0.0234(14) Uani 1 1 d . . .
H4A H 0.9176 0.1929 0.4089 0.028 Uiso 1 1 calc R . .
C5 C 1.0429(8) 0.3642(8) 0.3358(6) 0.0261(14) Uani 1 1 d . . .
C6 C 1.0404(8) 0.5099(8) 0.3003(5) 0.0236(14) Uani 1 1 d . . .
H6A H 1.1222 0.5597 0.2641 0.028 Uiso 1 1 calc R . .
C7 C 0.6567(7) 0.2751(7) 0.4602(5) 0.0220(13) Uani 1 1 d . . .
C8 C 0.278(2) 0.6736(19) 0.9973(12) 0.152(8) Uani 1 1 d . . .
H8A H 0.3555 0.6216 0.9721 0.227 Uiso 1 1 calc R . .
H8B H 0.1682 0.5938 0.9845 0.227 Uiso 1 1 calc R . .
H8C H 0.3204 0.7216 1.0768 0.227 Uiso 1 1 calc R . .
C9 C 0.1267(18) 0.854(2) 0.9517(11) 0.141(7) Uani 1 1 d . . .
H9A H 0.1301 0.9434 0.9138 0.211 Uiso 1 1 calc R . .
H9B H 0.1364 0.8909 1.0309 0.211 Uiso 1 1 calc R . .
H9C H 0.0207 0.7680 0.9195 0.211 Uiso 1 1 calc R . .
C10 C 0.3738(16) 0.8563(14) 0.8793(9) 0.081(3) Uani 1 1 d . . .
H10A H 0.3598 0.9437 0.8473 0.097 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O5 Pb1 O1W 79.73(18) 2_666 .
O5 Pb1 O6 115.39(14) 2_666 1_565
O1W Pb1 O6 76.65(18) . 1_565
O5 Pb1 O4 67.50(14) 2_666 .
O1W Pb1 O4 66.55(16) . .
O6 Pb1 O4 142.12(16) 1_565 .
O3 S1 O2 112.4(3) . .
O3 S1 O1 112.3(3) . .
O2 S1 O1 112.9(3) . .
O3 S1 C1 107.5(3) . .
O2 S1 C1 105.7(3) . .
O1 S1 C1 105.4(3) . .
Pb1 O1W H1W1 104(5) . .
Pb1 O1W H1W2 126(6) . .
H1W1 O1W H1W2 110.0(18) . .
H2W2 O2W H2W1 108.7 . .
H3W2 O3W H3W1 108.0 . .
C2 O4 Pb1 133.6(3) . .
C2 O4 H4O 105(5) . .
Pb1 O4 H4O 107(5) . .
C7 O5 Pb1 106.5(4) . 2_666
C7 O6 Pb1 164.4(4) . 1_545
C5 O7 H7O 110(6) . .
C10 N1 C8 124.3(13) . .
C10 N1 C9 122.1(13) . .
C8 N1 C9 113.5(12) . .
C6 C1 C2 120.2(6) . .
C6 C1 S1 120.3(5) . .
C2 C1 S1 119.5(5) . .
O4 C2 C3 121.1(5) . .
O4 C2 C1 118.6(5) . .
C3 C2 C1 120.3(5) . .
C2 C3 C4 118.9(5) . .
C2 C3 C7 120.7(5) . .
C4 C3 C7 120.5(5) . .
C5 C4 C3 121.7(6) . .
C5 C4 H4A 119.1 . .
C3 C4 H4A 119.1 . .
O7 C5 C4 118.1(6) . .
O7 C5 C6 123.0(6) . .
C4 C5 C6 118.9(6) . .
C1 C6 C5 119.9(6) . .
C1 C6 H6A 120.0 . .
C5 C6 H6A 120.0 . .
O6 C7 O5 121.9(5) . .
O6 C7 C3 121.0(5) . .
O5 C7 C3 117.0(5) . .
N1 C8 H8A 109.5 . .
N1 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
N1 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N1 C9 H9A 109.5 . .
N1 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N1 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
O8 C10 N1 123.9(12) . .
O8 C10 H10A 118.0 . .
N1 C10 H10A 118.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O5 2.452(4) 2_666
Pb1 O1W 2.453(5) .
Pb1 O6 2.528(4) 1_565
Pb1 O4 2.671(4) .
S1 O3 1.448(5) .
S1 O2 1.448(5) .
S1 O1 1.460(5) .
S1 C1 1.773(6) .
O1W H1W1 0.85(7) .
O1W H1W2 0.85(7) .
O2W H2W2 0.8500 .
O2W H2W1 0.8500 .
O3W H3W2 0.8500 .
O3W H3W1 0.8500 .
O4 C2 1.363(7) .
O4 H4O 0.85(7) .
O5 C7 1.263(7) .
O5 Pb1 2.452(4) 2_666
O6 C7 1.246(7) .
O6 Pb1 2.528(4) 1_545
O7 C5 1.362(7) .
O7 H7O 0.85(7) .
O8 C10 1.250(14) .
N1 C10 1.322(13) .
N1 C8 1.374(16) .
N1 C9 1.430(16) .
C1 C6 1.378(9) .
C1 C2 1.397(8) .
C2 C3 1.382(8) .
C3 C4 1.388(8) .
C3 C7 1.499(8) .
C4 C5 1.379(9) .
C4 H4A 0.9300 .
C5 C6 1.403(9) .
C6 H6A 0.9300 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 H10A 0.9300 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O3 0.85(7) 1.865(18) 2.699(7) 168(7) .
O1W H1W2 O2W 0.85(7) 1.90(3) 2.717(7) 162(8) 2_676
O2W H2W2 O8 0.85 1.87 2.711(10) 168.8 .
O2W H2W1 O2 0.85 1.83 2.665(8) 168.2 2_776
O3W H3W2 O8 0.85 2.01 2.839(11) 163.4 .
O3W H3W1 O4 0.85 2.28 3.103(8) 163.9 2_666
O3W H3W1 O1W 0.85 2.59 3.137(8) 123.2 2_666
O4 H4O O5 0.85(7) 1.70(4) 2.482(6) 150(7) .
O7 H7O O3W 0.85(7) 1.801(13) 2.653(7) 179(9) 2_766
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O5 Pb1 O4 C2 -143.6(5) 2_666 . . .
O1W Pb1 O4 C2 128.2(5) . . . .
O6 Pb1 O4 C2 113.5(5) 1_565 . . .
O3 S1 C1 C6 123.8(5) . . . .
O2 S1 C1 C6 3.6(6) . . . .
O1 S1 C1 C6 -116.2(5) . . . .
O3 S1 C1 C2 -56.8(6) . . . .
O2 S1 C1 C2 -177.0(5) . . . .
O1 S1 C1 C2 63.2(6) . . . .
Pb1 O4 C2 C3 121.2(5) . . . .
Pb1 O4 C2 C1 -59.1(7) . . . .
C6 C1 C2 O4 177.4(5) . . . .
S1 C1 C2 O4 -1.9(8) . . . .
C6 C1 C2 C3 -2.9(9) . . . .
S1 C1 C2 C3 177.8(5) . . . .
O4 C2 C3 C4 -177.4(5) . . . .
C1 C2 C3 C4 2.9(9) . . . .
O4 C2 C3 C7 2.8(9) . . . .
C1 C2 C3 C7 -176.9(6) . . . .
C2 C3 C4 C5 -0.8(10) . . . .
C7 C3 C4 C5 179.0(6) . . . .
C3 C4 C5 O7 177.8(6) . . . .
C3 C4 C5 C6 -1.4(10) . . . .
C2 C1 C6 C5 0.6(10) . . . .
S1 C1 C6 C5 180.0(5) . . . .
O7 C5 C6 C1 -177.7(6) . . . .
C4 C5 C6 C1 1.5(10) . . . .
Pb1 O6 C7 O5 166.6(13) 1_545 . . .
Pb1 O6 C7 C3 -10(2) 1_545 . . .
Pb1 O5 C7 O6 -18.8(8) 2_666 . . .
Pb1 O5 C7 C3 157.7(4) 2_666 . . .
C2 C3 C7 O6 178.8(6) . . . .
C4 C3 C7 O6 -1.0(9) . . . .
C2 C3 C7 O5 2.2(9) . . . .
C4 C3 C7 O5 -177.6(6) . . . .
C8 N1 C10 O8 5.5(19) . . . .
C9 N1 C10 O8 -178.9(11) . . . .
